CN101222983B - 用于在常压等离子体中疏水和超疏水处理的表面涂覆方法 - Google Patents
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Abstract
本发明涉及一种使用常压等离子体在工件表面涂覆碳氟化合物或烃的方法。更特别的,本发明涉及一种使用在常压产生的等离子体在工件表面涂覆烃或碳氟化合物从而使得该工件可以具有疏水性或超疏水性表面的方法。根据本发明采用碳氟化合物将工件表面涂覆成疏水的或超疏水的的方法包括步骤,通过将一种反应气体供入一个形成在第一电极和第二电极之间的放电空间,产生第一常压辉光等离子体,该反应气体包括氢气、碳氟化合物气体和惰性气体,第一和第二电极被连接到一个常压等离子体发生器的RF电源;将该工件靠近流过该放电空间的反应气体下游的第一电极,由此,在该放电空间产生的等离子体被传递到第一电极和该工件之间的空间,以在其中产生第二常压辉光等离子体,借此,一种碳氟化合物涂层可被形成在该工件的表面上。
Description
技术领域
本发明涉及一种使用常压等离子体在工件表面上涂覆碳氟化合物或烃的方法。更具体地,本发明涉及一种使用在常压下所产生的等离子体在工件表面上涂覆烃或碳氟化合物,使得该工件能够具有疏水性或超疏水性表面的方法。
背景技术
疏水性是指一种表示水与物体之间相互作用的化学性能,即概念上不具有对水的亲和力。
图13所表示的是水与物体表面之间的接触角。越高的接触角表示越高的疏水趋势。例如,180度的接触角意味着该物体表面被处理成为超疏水性。在这种情况下,水在该物体表面上保持为完美球形。
通常,疏水性材料容易在自然界中找到。芋头叶或荷叶是典型的疏水性材料。Wenzel′s和Cassie′s已经发现,叶子表面上的疏水性归因于其表面上的多微孔结构。图14所述的是具有疏水性的植物叶子及其多微孔结构。
化学或物理方法可以用来将物体的表面处理成为疏水的或超疏水的。
图15所示的是通过物理方法改性的物体的表面结构的例子。为了提供超疏水性,在该物体的光滑表面上使用碳纳米管形成多孔结构。如果水滴落在所述碳纳米管的表面上,则它将保持为接近球形的形式。
化学方法包括在物体的表面上应用含氟涂层等,例如,在制造煎锅时。也就是说,物体表面的化学组成被转变成使该表面为疏水或超疏水的。特别是,在其它的化学材料中,氟烷聚合物显示出强的疏水趋势。
美国专利4,869,922、6,649,222和5,733,610公开了将物体表面处理成疏水性或超疏水性的化学方法。
美国专利4,869,922公开了一种使用真空等离子体在物体表面上涂覆多氟烃以显示出疏水性的表面处理方法。在该专利中,在1托的压力下将氢气与单体C-F气体的混合物注入到放电空间中。此外,施加40~80W的27.12MHz的RF(射频)功率5~20分钟,以在20×20×1mm的铝样品的表面上涂覆多氟烃,由此该样品的表面可以被改性成疏水的。
美国专利6,649,222公开了一种使用调制的辉光放电等离子体将样品的表面处理成超疏水性的方法。在300~400毫托的压力下,施加50~75W的13.56MHz调制频率20~90分钟,单体C-F气体被用来处理具有2-20cm2面积的非金属样品如PE、PP、硅、玻璃和PET的表面。
美国专利5,733,610公开了一种在常压下提供疏水性的表面处理方法。在常压下使用3000Hz的频率处理有机样品和硅晶片样品的表面。
使用真空系统将表面处理成疏水性或超疏水性的传统方法只能在封闭系统中进行。因此,该传统方法不能实现连续或自动的方法,其中,样品被移动且同时被处理,因此,存在一个问题,该技术不能被用于大规模工业生产。
进一步地,用于真空系统的昂贵真空设备及其相应的维护导致成本的增加。
另外,由于聚合物在高温下会改变它们的性质,所以它们应该在较低的温度下和在几秒钟的时间内被处理。因此,存在另一个问题,难以控制用于精细处理的加工条件。
此外,存在进一步的问题,在常压下将目标表面处理成疏水性的方法应该采用一批抑制电弧产生的系统。
发明内容
技术问题
本发明已经设想解决在将物体表面处理成疏水性或超疏水性的传统方法中的上述问题。本发明的一个目的在于提供一种在常压下不使用真空系统将物体表面处理成疏水性或超疏水性的方法。
本发明的另一个目的在于提供一种在常压下不使用洗浴系统(bathsystem)处理物体表面的方法。
技术方案
根据本发明的一个方面,提供一种用碳氟化合物将工件的表面涂覆成疏水性或超疏水性的方法,该方法包括步骤:通过将一种反应气体供应到形成于第一电极和第二电极之间的放电空间,产生第一常压辉光等离子体,所述反应气体包含氢气、碳氟化合物气体和惰性气体,所述第一电极和所述第二电极被连接到常压等离子体发生器的RF电源;以及将该工件靠近流过该放电空间的反应气体的下游的第一电极,所以,在该放电空间中所产生的等离子体被传送到第一电极和所述工件之间的空间,以在其中产生第二常压辉光等离子体,由此,在该工件的表面上形成碳氟化合物涂层。优选地,碳氟化合物气体选自以下气体组成的组:CF3、CF4、C2F6、C4F8及其混合物,在反应气体中所含的碳氟化合物气体和氢气的体积比(碳氟化合物/氢)在0.1~10的范围内。优选地,反应气体中所含的惰性气体的体积为该反应气体的总体积的至少90%,惰性气体包括氦气,且氦气的体积为惰性气体总体积的至少60%。更优选地,采用在100KHz~60MHz频率下运行的RF电源以产生等离子体,所述工件靠近第一电极至1~10mm的范围内。
在本发明的表面涂覆方法中,等离子体发生器的第一电极采取具有预定长度的棒的形状;第二电极与第一电极沿着第一电极的纵向间隔预定距离,由此在电极之间形成放电空间;等离子体发生器进一步包括用通道形成的气体供应单元,通过所述通道,所述反应气体可以被供应到所述放电空间中;所述通道包括沿第一电极的纵向形成的缓冲空间、沿第一电极纵向形成且具有朝着放电空间开放的一侧的混合空间、和用于使所述缓冲空间和所述混合空间的内壁彼此相通的孔。在这种情况中,所述等离子体发生器可以进一步包括与第一电极相连的电容器。
可选择地,在本发明的表面涂覆方法中,等离子体发生器的第一电极采取具有预定长度的棒的形状;第二电极与第一电极沿着第一电极的纵向间隔预定距离,以在电极之间形成放电空间;等离子体发生器进一步包括用通道形成的气体供应单元以及与第一电极相连的电容器,通过所述通道,所述反应气体可以被供应到所述放电空间。
根据本发明的另一方面,提供用碳氟化合物将工件表面涂覆成疏水性或超疏水性的方法,该方法包括步骤:通过将反应气体供应到形成于第一电极和第二电极之间的放电空间,产生第一常压辉光等离子体,所述反应气体包含烃气体、碳氟化合物气体和惰性气体,所述第一电极和所述第二电极与被连接到常压等离子体发生器的RF电源;以及将工件靠近流过所述放电空间的反应气体的下游的第一电极,所以在该放电空间中所产生的等离子体被传送到第一电极和所述工件之间的空间,以在其中产生第二常压辉光等离子体,由此,在该工件的表面上形成碳氟化合物涂层。在这种情况中,优选地,烃气体选自以下气体组成的组:C2H2、CH4、C2H4、C2H6、C3H8及其混合物,碳氟化合物气体选自以下气体组成的组:CF3、CF4、C2F6、C4F8及其混合物。进一步地,优选反应气体中所含的碳氟化合物气体和烃气的体积比(碳氟化合物/烃)在0.1~10的范围内,反应气体中所含的惰性气体的体积为该反应气体的总体积的至少90%。优选地,惰性气体包括氦气,且氦气的体积为惰性气体的总体积的至少60%。
采用在100KHz~60MHz频率运行的RF电源以产生等离子体。优选地,工件靠近第一电极至在1~10mm范围内。
根据本发明的另一方面,提供一种用碳氟化合物将工件表面涂覆成疏水性或超疏水性的方法,该方法包括步骤:通过提供包含氢气、碳氟化合物气体和惰性气体的反应气体给常压等离子体发生器,产生常压辉光等离子体;以及将工件的表面暴露于所产生的常压辉光等离子体中,从而在该工件表面上形成碳氟化合物涂层。优选地,碳氟化合物气体选自以下气体组成的组:CF3、CF4、C2F6、C4F8及其混合物,反应气体中所含的碳氟化合物气体和氢气的体积比(碳氟化合物/氢)在0.1~10范围内。优选地,反应气体中所含的惰性气体的体积为该反应气体的总体积的至少90%,惰性气体包括氦气,且氦气的体积为惰性气体的总体积的至少60%。另外,在辉光等离子体产生步骤中,所述常压等离子体发生器可以使用在100KHz~60MHz频率下运行的RF电源。
根据本发明的另一方面,提供一种用碳氟化合物将工件表面涂覆成疏水性或超疏水性的方法,该方法包括步骤:通过提供包含烃气体、碳氟化合物气体和惰性气体的反应气体给常压等离子体发生器,产生常压辉光等离子体;以及将工件的表面暴露于所产生的常压辉光等离子体,从而在该工件表面上形成碳氟化合物涂层。优选地,碳氟化合物气体选自以下气体组成的组:CF3、CF4、C2F6、C4F8及其混合物,烃气体选自以下气体组成的组:C2H2、CH4、C2H4、C2H6、C3H8及其混合物。优选地,反应气体中所含的碳氟化合物气体和烃气体的体积比(碳氟化合物/烃)在0.1~10范围内,反应气体中所含的惰性气体的体积为该反应气体的总体积的至少90%,惰性气体包括氦气,且氦气的体积为惰性气体的总体积的至少60%。采用在100KHz~60MHz频率下运行的RF电源以产生等离子体。
根据本发明的另一方面,提供一种用烃涂覆工件表面的方法,该方法包括步骤:通过将反应气体供应到形成于第一电极和第二电极之间的放电空间,产生第一常压辉光等离子体,所述反应气体包括烃气体和惰性气体,第一电极和第二电极被连接到常压等离子体发生器的RF电源;以及将工件靠近流过所述放电空间的反应气体的下游的第一电极,所以在该放电空间所产生的等离子体被传送到第一电极和所工件之间的空间,以在其中产生第二常压辉光等离子体,由此,在该工件的表面上形成烃涂层。优选地,烃气体选自以下气体组成的组:C2H2、CH4、C2H4、C2H6、C3H8及其混合物,惰性气体的体积为反应气体的总体积的至少90%。更优选地,选自氦、氩及其混合物的气体的体积为惰性气体的总体积的至少60%。
在本发明的表面涂覆方法中,等离子体发生器的第一电极采取具有预定长度的棒的形状;第二电极与第一电极沿着第一电极的纵向间隔预定距离,以在电极之间形成放电空间;等离子体发生器进一步包括用通道形成的气体供应单元,通过所述通道,反应气体可被供应到放电空间;所述通道包括沿着第一电极的纵向形成的缓冲空间、沿着第一电极的纵向形成且具有朝着放电空间开放的一侧的混合空间、和用于使所述缓冲空间和所述混合空间的内壁彼此相通的孔。等离子体发生器可以进一步包括与第一电极相连的电容器。
可选择地,在本发明的表面涂覆方法中,等离子体发生器的第一电极采取具有预定长度的棒的形状;第二电极与第一电极沿着第一电极的纵向间隔预定距离,以在电极之间形成放电空间;等离子体发生器进一步包括用通道形成的气体供应单元以及与第一电极相连的电容器,通过所述通道,反应气体可被供应到所述放电空间。
附图说明
图1为根据本发明的第一实施方式的常压等离子体发生器的示意图;
图2为本发明的常压等离子体发生器中的辊对辊型样品供应单元的概念视图;
图3为本发明的常压等离子体发生器中的卷对卷型样品供应单元的概念视图;
图4为根据本发明的第二实施方式的常压等离子体发生器的示意图;
图5所示的是根据本发明处理的工件的FTIR分析数据;
图6所示的是根据本发明处理的工件的并且通过处理次数分类的FTIR分析数据;
图7为沉积在金膜上的超疏水涂层的XPS谱;
图8所示的是用CF4-H2-He气体处理的金膜的AFM图;
图9所示的是根据本发明的实施方式处理成超疏水性的工件的接触角图;
图10所示的是根据本发明的实施方式处理成疏水性的工件的接触角图;
图11所示的是水滴落在根据本发明的实施方式处理成超疏水性的膜上的图;
图12所示的是水滴落在根据本发明的实施方式处理成超疏水性的膜上的图像和E-SEM图像;
图13所示的是水和物体的表面之间的接触角的例子;
图14所示的是具有疏水性的植物叶子及其多孔结构;
图15所示的是使用碳纳米管处理的物体的疏水性表面结构的例子。
具体实施方式
下文将参照附图,详细描述根据本发明的优选实施方式将工件表面处理成疏水性或超疏水性的方法。
图1解释了用于根据本发明将工件表面处理成疏水性或超疏水性的常压等离子体发生器的构造。
常压发生器包括RF电源400、等离子体模块405、匹配箱401、样品供应单元421和气体供应单元。
RF电源400提供将反应气体电离成等离子态所需要的电能,匹配箱401将来源于RF电源400的电能以处于稳定频率波段的电能形式供应给等离子体模块405。
气体供应单元包括气体供应管410、411和412以及气体混合器413。气体供应管410、411和412供应用于产生等离子体和将工件表面处理成疏水性或超疏水性所需要的气体。可选择地,气体供应管可以包括多个管。气体混合器413使通过气体供应管410、411和412被引入的气体混合成为反应气体,该反应气体随后被供应给等离子体模块405。
等离子体模块405包括第一电极402、第二电极403、电介质404、气体供应通道407和放电空间406。
第一电极402与匹配箱401连接用于接收来自RF电源400的电能,并被电介质404覆盖。第二电极403接地并与第一电极402间隔某一距离,以形成电极之间的放电空间406。气体供应通道407容纳来自于气体混合器413的反应气体,并将反应气体供应到放电空间406中。在反应气体被引入到放电空间406之后,然后电能被提供给第一电极402,通过第一电极402和第二电极403之间的电压,反应气体在放电空间406内辉光放电并且同时转化为等离子态。
样品供应单元421在第一电极402之下提供将被表面处理的工件420。在放电空间406内所产生的等离子态的反应气体在第一电极402下流动。此时,如果工件420被放置在第一电极402之下处于放电空间406的出口侧,在该工件420的表面上方就会发生等离子体转化现象。
用于提供工件420的方法包括扫描法、辊对辊法(roll-to roll method)、卷对卷法(reel-to-reel)等。
图2所示的是一种通过辊对辊法在第一电极500之下提供工件502的方法。工件502通过辊503来运送,并且直接暴露于在第一电极500和接地电极504之间传送的等离子体,由此,它可以被处理成疏水性或超疏水性。此时,电极和工件之间的距离大约为1~10mm。接地电极504被置于稍低于所述辊的位置,由此,在工件和接地电极504之间产生间隙505。因此,工件可以以其底面不与接地电极504发生接触的状态下被顺利地运送。
图3所示的是一种通过卷对卷法在第一电极600之下提供工件602的方法。工件602通过辊603来运送,并且直接暴露于在第一电极600和接地电极604之间传送的等离子体601,由此,它可以被处理成疏水性或超疏水性。
RF电源具有100KHz~60MHz的工作频率,并且通过匹配箱401在稳定的频率波段下将RF功率应用于电极。第一电极被电介质404覆盖,由此,没有电弧产生且可以防止工件的损坏。
用于将工件的表面处理成疏水性和超疏水性的反应气体由惰性气体和工作气体组成。惰性气体优选为氦气,可以进一步包括氩气、氖气等。惰性气体优选具有不低于所述反应气体的总体积的90%,更优选地为95.00-99.99%。此外,优选惰性气体的体积的至少60%填充氦气。
为了将工件表面处理成疏水性或超疏水性(例如,达到接触角不小于150°的程度),烃气和碳氟化合物气体被用作工作气体。优选地,所述烃气体选自以下组成的组:C2H2、CH4、C2H4、C2H6、C3H8及其混合物,碳氟化合物气体选自以下组成的组:CF3、CF4、C2F6、C4F8及其混合物。作为工作气体,氢气或SiH4气体可以被用来代替烃气,SF6气体也可以被用来代替碳氟化合物气体。
另外,碳氟化合物气体的体积优选控制在氢气或烃气体积的0.1~10倍。当工件表面暴露于等离子态的反应气体时,碳氟化合物以多氟烃的形式被涂覆在工件表面上,所以该工件显示出疏水性或超疏水性。此时,烃基气体构成了涂覆环境。
其它的用于将工件表面处理成疏水性的工作气体包括烃气。当工件表面暴露于等离子态的反应气体时,烃被涂覆在工件表面上,所以该工件显示出疏水性。
当等离子体430在反应空间406产生时,工件420在第一电极402之下通过样品供应单元422进行运送和传递,等离子体被传递和直接暴露于工件420。根据所使用的反应气体,工件420可以被处理成疏水性或超疏水性。工件420可以被在停顿状态下处理或者重复处理。通常,在工件小于等离子体产生区的情况下,工件可以被在停顿状态下或重复进行等离子体处理。
图4所示的是根据本发明另一实施方式的等离子体发生器。在该实施方式的常压等离子体发生器中,第一电极组件30与高频电源40电连接,用于通过匹配箱41提供高频功率。第二电极15与第一电极组件30间隔预定距离,以在所述电极之间形成放电空间15a。形成有入口11的气体供应单元10被构造为夹持和支撑第一电极组件30和第二电极15,通过所述入口11,反应气体可以被供应到第一电极组件30和第二电极15之间的放电空间15a。工件M被放置在流经放电空间15a的反应气体的下游,并且与第一电极组件30间隔预定距离。气体供应单元10的入口11被构造为与在第一电极装置30的纵向上形成的缓冲空间12相连接。进一步地,气体供应单元10形成有混合空间13a,其沿着第一电极组件30的纵向形成,且与缓冲空间12间隔某一距离,并且与放电空间15a相连接。另外,气体供应单元10具有多个孔13,其将混合空间13a和缓冲空间12相互连通。此外,第一电极组件30是一种长的元件,其一侧(在该图中由虚线表示)连接到电源,另一侧进行电连接,并且与电容连接接地。第一电极装置30包括导体32和沿导体32外周卷绕的硅树脂31。
当通过气体供应单元10的入口11供应反应气体时,如果RF功率被用于第一电极装置30,第一等离子体P1首先在放电空间15a内产生。由于第一电极装置和第二电极之间的距离小于第一电极装置和工件M表面之间的距离,产生在放电空间15a内的等离子体P1可以容易地被传送到工件M和第一电极装置之间的空间,从而产生用于稳定的表面处理的等离子体P2。特别是,由于电连接到第一电极装置的导体一侧端的电容C1接地,沿第一电极装置纵向的不均匀的电压分布可以被防止,从而产生稳定的等离子体P1和P2。电容C1允许通过充电和放电操作而使得第一电极装置上的电压是均匀分布的。由于高频功率的应用,电容即使不接地也可以被充电和放电。然而,优选电容接地。另外,通过入口11供应的反应气体沿着缓冲空间12的纵向具有初级均匀的压力分布,所述缓冲空间12沿着第一电极组件30的纵向形成。在均匀的压力下,通过多个孔13从缓冲空间12提供的反应气体碰撞混合空间13的内壁,然后,在混合空间内混合以使其沿着第一电极组件30的纵向具有第二均匀压力分布。在混合空间13中的反应气体具有均匀压力分布,其被供应到放电空间15a,所以稳定的等离子体P1和P2可以沿着第一电极组件30的纵向产生。
在该实施方式的等离子体发生器中,等离子体在放电空间内产生,然后被传送到工件表面上,由此,可以在工件表面上涂覆多氟烃或烃。然而,所述工件可被直接运送到产生等离子体的放电空间,以实施表面处理。
所述工件可以是金属材料、玻璃、硅晶片、氧化物、氮化物、陶瓷、聚合物、橡胶、硅树脂和纤维或其复合材料中的一种,除了液体和气体之外。
实施例
下文将详细描述本发明的实施例。
实施例1
目的:超疏水性 惰性气体:He(10升/分钟)
频率:13.56MHz 反应气体:CF4(15sccm(立方厘米/分钟)),H2(5sccm)
功率:250W 处理次数:15次
工件:铜片 处理速率:10毫米/秒
处理后的接触角:171°
实施例2
目的:超疏水性 惰性气体:He(10升/分钟)
频率:13.56MHz 反应气体:CF4(15sccm),CH4(5sccm)
功率:250W 处理次数:15次
工件:铝片 处理速率:10毫米/秒
处理后的接触角:168°
实施例3
目的:超疏水性 惰性气体:He(10升/分钟),Ar(1升/分钟)
频率:13.56MHz 反应气体:CF4(10sccm),H2(5sccm)
功率:250W 处理次数:10次
工件:玻璃 处理速率:10毫米/秒
处理后的接触角:157°
实施例4
目的:超疏水性 惰性气体:He(10升/分钟)
频率:13.56MHz 反应气体:CF4(10sccm),H2(5sccm)
功率:250W 处理次数:20次
工件:聚酰亚胺膜 处理速率:10毫米/秒
处理后的接触角:175°
实施例5
目的:疏水性 惰性气体:He(10升/分钟)
频率:13.56MHz 反应气体:CH4(10sccm)
功率:200W 处理次数:10次
工件:铜片 处理速率:10毫米/秒
处理后的接触角:112°
实施例6
目的:疏水性 惰性气体:He(10升/分钟)
频率:13.56MHz 反应气体:CH4(10sccm)
功率:200W 处理次数:10次
工件:玻璃 处理速率:10毫米/秒
处理后的接触角:115°
在实施例1到6中,氦被用作惰性气体以将工件表面处理成疏水性或超疏水性。金属、基于聚合物的膜和玻璃被用作工件。然而,由于所述处理是在常压下进行的,在真空方法中可能引起问题的排气无须考虑。从而,包括上述实施例描述的工件材料的各种材料都可以用作工件。
另外,由于等离子体具有鞘状面,本发明可以被用于各种工件如平板、针、大块型、表面、颗粒等的表面处理。
图5所示的是根据本发明的工件的FTIR数据。位于特定波长波段的顶点表示相关元素的结合形式和结合能。作为分析结果,已经发现CF2-、CF3-和CF-基多氟烃被涂覆在工件上。
图6所示的是根据本发明处理的工件的并且通过处理次数分类的FTIR数据。从图中可以看出,C-F基和C-C基元件的信号强度随处理次数的增加而增加。
图7所示的是沉积在金膜上的超疏水性涂层的XPS能谱。所测量的能谱对应于处理三次的涂层。C1s和F1s的高分辨率谱分别对应于处理三次和九次的涂层。作为将高分辨率谱分析成具有多个顶点的能谱的结果,可以看出,已经检测到具有各种结合能的碳-基和氟-基元素。所插入的数子表示处理的次数。为了将C-C置于285.0eV,C1s和F1s能谱通过所希望的数量进行补偿。
图8所示的是根据处理次数使用CF4-H2-He气体处理金膜的AFM图象,其中,(a)对应于未处理金膜的图象,而(b)、(c)、和(d)分别对应于金膜被处理三次、七次和十一次的图象。用于各个图象的对照物的尺寸为(a)14.4nm、(b)44.6nm、(c)64.0nm和(d)79.6nm。
从该图中可以看出,表面粗糙度随处理次数的增加而增加。进一步地,在十一次处理之后,可以获得次纳米级表面粗糙度。考虑到在真空方法中处理工件,当其表面粗糙度为微米级时,可获得超疏水性,可以看出,按照本发明的工件的表面,即使当它具有极低的表面粗糙度时,也显示出超疏水性。
图9所示的是由(a)铜、(b)硅晶片、(c)铝和(d)玻璃载片制成的工件的接触角,其根据本发明的实施方式被处理成疏水性。处理速率和处理次数分别为10毫米/秒和10次。
图10所示的是由(a)铜、(b)硅晶片、(c)棉、(d)纸和(e)玻璃载片制成的工件的接触角,其根据本发明的实施方式被处理成疏水性。处理速率和处理次数分别为10毫米/秒和10次。
图11所示的是水滴落在金膜(上图)和棉织物(下图)上的连续图象,其根据本发明的实施方式被涂覆成超疏水性。前六个图象每间隔2ms拍摄一次,剩余两个图象每间隔6ms拍摄一次。落在超疏水性工件上的水滴不仅没有粘附该到工件上,而且从该工件上弹起来。
图12(a)是表示水滴落在根据本发明的实施方式被处理成超疏水性金膜上的照片,图12(b)和(c)是表示在沉积于金膜的超疏水性涂层膜上冷凝的水滴的E-SEM图。蒸气压为5.54托,工件的温度为3.0℃,图12(b)和(c)中的比例尺分别为100mm和5mm。
工业实用性
根据本发明,使用常压辉光放电等离子体将工件表面处理成疏水性或超疏水性。通过调整处理速率和处理次数,容易改性所述工件的表面。
另外,根据工件的类型,不同的运输系统如扫描型、辊对辊型和卷对卷型可以被选择用于控制多氟烃的沉积速率。由于大面积的工件可以通过使用连续的工艺处理,对需要处理的工件的尺寸没有限制。
此外,在开放空间采用常压等离子体处理与采用真空等离子体处理相比较,具有较高的处理速率。因此,可以减少时间和节约成本,还可以提高产品的产量。
尽管本发明已经采用优选的实施方式描述并在附图中进行了解释,但是本发明并不因此而被限制,而是由附加的权利要求来定义。因此,对于本领域技术人员而言,可以容易地理解,在不脱离由附加权利要求定义的本发明的精神和范围的情况下,可以得到各种改进和修改。
Claims (27)
1.一种用碳氟化合物涂覆工件的表面的方法,包括步骤:
通过将反应气体供应到形成于第一电极和第二电极之间的放电空间,产生第一常压辉光等离子体,所述反应气体包含氢气、碳氟化合物气体和惰性气体,第一电极和第二电极与常压等离子体发生器的RF电源相连;以及
将工件靠近在流过所述放电空间的反应气体的下游的第一电极,使得在所述放电空间中产生的等离子体被传送到第一电极和所述工件之间的空间,以在其中产生第二常压辉光等离子体,由此,在所述工件的表面上形成碳氟化合物涂层。
2.如权利要求1的方法,其中,所述碳氟化合物气体选自以下组成的组:CF3、CF4、C2F6、C4F8及其混合物。
3.如权利要求1或2的方法,其中,所述反应气体中含有的碳氟化合物气体和氢气的体积比(碳氟化合物/氢)在0.1~10范围内。
4.如权利要求3的方法,其中,所述反应气体中含有的惰性气体的体积为该反应气体的总体积的至少90%。
5.如权利要求4的方法,其中,所述惰性气体包括氦气,氦气的体积为该惰性气体的总体积的至少60%。
6.如权利要求1的方法,其中,使用在100KHz~60MHz频率下运行的RF电源来产生等离子体。
7.如权利要求6的方法,其中,所述工件靠近第一电极至1~10mm范围内。
8.如权利要求5的方法,其中,使用在100KHz~60MHz频率下运行的RF电源来产生等离子体,并且所述工件靠近第一电极至1~10mm范围内。
9.如权利要求1的方法,其中:
所述等离子体发生器的第一电极采取具有预定长度的棒的形状;
第二电极与第一电极沿着第一电极的纵向间隔预定距离,由此在所述电极之间形成放电空间;
所述等离子体发生器进一步包括用通道形成的气体供应单元,通过该通道,所述反应气体可以被供应到所述放电空间中;以及
所述通道包括沿着第一电极的纵向形成的缓冲空间、沿着第一电极的纵向形成且具有朝着放电空间开放的一侧的混合空间、和用于使所述缓冲空间和所述混合空间的内壁彼此相通的孔。
10.如权利要求1的方法,其中:
所述等离子体发生器的第一电极采取具有预定长度的棒的形状;
第二电极与第一电极沿着第一电极的纵向间隔预定距离,以在所述电极之间形成放电空间;以及
所述等离子体发生器进一步包括用通道形成的气体供应单元以及与第一电极相连的电容器,通过所述通道,所述反应气体可以被供应到所述放电空间中。
11.如权利要求9的方法,其中,所述等离子体发生器进一步包括与第一电极相连的电容器。
12.一种用碳氟化合物涂覆工件的表面的方法,包括步骤:
通过将反应气体供应到形成于第一电极和第二电极之间的放电空间,产生第一常压辉光等离子体,所述反应气体包括烃气体、碳氟化合物气体和惰性气体,第一电极和第二电极与常压等离子体发生器的RF电源相连;以及
将工件靠近流过所述放电空间的反应气体的下游的第一电极,使得在所述放电空间中产生的等离子体被传送到第一电极和工件之间的空间,以在其中产生第二常压辉光等离子体,由此,在该工件的表面上形成碳氟化合物涂层。
13.如权利要求12的方法,其中,所述烃气体选自以下组成的组:C2H2、CH4、C2H4、C2H6、C3H8及其混合物。
14.如权利要求13的方法,其中,所述碳氟化合物气体选自以下组成的组:CF3、CF4、C2F6、C4F8及其混合物。
15.如权利要求12-14中任一项的方法,其中,所述反应气体中含有的碳氟化合物气体和烃气体的体积比(碳氟化合物/烃)在0.1~10范围内。
16.如权利要求15的方法,其中,所述反应气体中含有的惰性气体的体积为该反应气体的总体积的至少90%。
17.如权利要求16的方法,其中,所述惰性气体包括氦气,氦气的体积为该惰性气体的总体积的至少60%。
18.如权利要求12的方法,其中,使用在100KHz~60MHz频率下运行的RF电源来产生等离子体。
19.如权利要求18的方法,其中,所述工件靠近第一电极至1~10mm范围内。
20.如权利要求17的方法,其中,使用在100KHz~60MHz频率下运行的RF电源来产生等离子体,并且所述工件靠近第一电极至1~10mm范围内。
21.一种用烃涂覆工件的表面的方法,包括步骤:
通过将反应气体供应到形成于第一电极和第二电极之间的放电空间,产生第一常压辉光等离子体,所述反应气体包含烃气体和惰性气体,第一电极和第二电极与常压等离子体发生器的RF电源相连;以及
将工件靠近流过所述放电空间的反应气体的下游的第一电极,使得在所述放电空间中产生的等离子体被传送到第一电极和工件之间的空间,以在其中产生第二常压辉光等离子体,由此,在该工件的表面上形成烃涂层。
22.如权利要求21的方法,其中,所述烃气体选自以下组成的组:C2H2、CH4、C2H4、C2H6、C3H8及其混合物。
23.如权利要求22的方法,其中,所述惰性气体的体积为所述反应气体的总体积的至少90%。
24.如权利要求23的方法,其中,选自氦、氩及其混合物的气体的体积为所述惰性气体的总体积的至少60%。
25.如权利要求21-24中任一项的方法,其中:
等离子体发生器的第一电极采取具有预定长度的棒的形状;
第二电极与第一电极沿着第一电极的纵向间隔预定距离,以在所述电极之间形成放电空间;
所述等离子体发生器进一步包括用通道形成的气体供应单元,通过该通道,所述反应气体可以被供应到所述放电空间中;以及
所述通道包括沿着第一电极的纵向形成的缓冲空间、沿着第一电极的纵向形成且具有朝着放电空间开放的一侧的混合空间、和用于使所述缓冲空间和所述混合空间的内壁彼此相通的孔。
26.如权利要求21-24中任一项的方法,其中:
等离子体发生器的第一电极采取预定长度的棒的形状;
第二电极与第一电极沿着第一电极的纵向间隔预定距离,以在所述电极之间形成放电空间;以及
所述等离子体发生器进一步包括用通道形成的气体供应单元以及与第一电极相连的电容器,通过所述通道,所述反应气体可以被供应到所述放电空间中。
27.如权利要求25的方法,其中,所述等离子体发生器进一步包括与第一电极相连的电容器。
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JP3720408B2 (ja) * | 1994-03-18 | 2005-11-30 | サムコ株式会社 | ハロゲン化炭化水素ガス処理方法及び装置 |
JPH09208726A (ja) * | 1996-02-02 | 1997-08-12 | Sekisui Chem Co Ltd | プラズマを利用した基材の表面処理方法 |
US6649222B1 (en) * | 1998-09-07 | 2003-11-18 | The Procter & Gamble Company | Modulated plasma glow discharge treatments for making superhydrophobic substrates |
US6652069B2 (en) * | 2000-11-22 | 2003-11-25 | Konica Corporation | Method of surface treatment, device of surface treatment, and head for use in ink jet printer |
US7887889B2 (en) * | 2001-12-14 | 2011-02-15 | 3M Innovative Properties Company | Plasma fluorination treatment of porous materials |
KR20040095104A (ko) * | 2003-05-06 | 2004-11-12 | 사단법인 고등기술연구원 연구조합 | 경표면 소재 도금 전처리용 상압 플라즈마 표면처리장치및 방법 |
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CN101222983A (zh) | 2008-07-16 |
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KR20070006991A (ko) | 2007-01-12 |
US20100221452A1 (en) | 2010-09-02 |
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